関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4,4,4-Trifluoro-3-[3-(3-trifluoromethylphenyl)-piperidin-1-ylmethyl]-butyric acid ethyl ester | HCID 90103432 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4,4,4-Trifluoro-3-((3-(3-(trifluoromethyl)phenyl)piperidin-1-yl)methyl)butanoic acid | HCID 90103570 | 99.1% |
反応手順
In a 10 mL pear-shaped flask, 4,4,4-trifluoro-3-[3-(3-trifluoromethyl-phenyl)-piperidin-1-ylmethyl]-butyric acid ethyl ester (130 mg, 316 μmol) and NaOH (237 μl, 474 μmol) were combined with ethanol (6 ml) to give a colorless solution. The reaction mixture was heated at 90° C. and stirred for 30 min. The reaction mixture was concentrated and treated with a saturated solution of NaH2PO4 (20 ml) and extracted with ethyl acetate (2×30 ml). The combined organics were washed with brine and H2O, dried over MgSO4, filtered and concentrated to give 120 mg (99%) of 4,4,4-trifluoro-3-[3-(3-trifluoromethyl-phenyl)-piperidin-1-ylmethyl]-butyric acid as a waxy solid. MH+=384.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09388172B2 |
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| 出典データセット | uspto-grants-2016_07 |
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| ORD ID | ord-74445e613e054f73a856921ad92a1545 |
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| 出典メモ | uspto-grants-2016_07 |
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